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Dimethylamine → HCID 22643244、化合物

HRID 2414765
ノート
印刷プレビュー

反応式

HRID 2414765 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1)[CH:8]=[C:7]2Cl)([O-:3])=[O:2].[CH3:22][NH:23][CH3:24].O>CN1C(=O)CCC1>[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1)[CH:8]=[C:7]2[N:23]([CH3:24])[CH3:22])([O-:3])=[O:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 674DimethylamineHCID 962WaterHCID 22643158HCID 22643158、化合物

生成物 1

HCID 22643244HCID 22643244、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
60 °C

実験手順

6-Nitro-4-chloro-2-(3-fluoro-phenyl)-quinoline, 20 g (59.4 mmoles), was placed in a 500 mL three-neck round-bottom flask equipped with magnetic stirrer, nitrogen inlet, gas outlet, condenser and heating bath. The material was dissolved in 150 mL of N-methyl pyrrolidinone, stirred and 250 mL of a 40% aq. solution of dimethylamine was added. The mixture was then warmed to 60° C. for 48 hrs. At the end of this time the reaction was cooled, poured into 3 L of water in a 4 L Erlenmeyer flask and the mixture stirred until solids formed. The solids were collected by vacuum filtration and dried in a vacuum oven. The product was recrystallised from-ethanol in a −20° C. freezer to give 19.6 g (95%) yield of the desired product.

後処理

  1. customequipped with magnetic stirrer, nitrogen inlet, gas outlet, condenser
  2. temperatureheating bath
  3. temperatureAt the end of this time the reaction was cooled
  4. stirringthe mixture stirred until solids
  5. customformed
  6. filtrationThe solids were collected by vacuum filtration
  7. customdried in a vacuum oven
  8. customThe product was recrystallised from-ethanol in a −20° C. freezer

出典と根拠

ORDレコード
ord-6cdd442b9a644d7ea210f2b7b28cfa25
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06815447B2

反応ノート

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